Separation of liquids



Feb. 4, 1941.

J. LOUMIET ET LAVIGNE SEPARATION OF LIQUIDS Filed Feb. 18, 1957 '7 Sheets-Sheet 1 l INVENTQR. Jean Loum/e e Ldv/gne.

ATTORNEYS.

Feb 4, 1941- J. LouMn-:T ET I AvlGNa 2,230,253

' SEPARATION OF LIQUIDS Filed Feb. 18, 1937 7 Sheets-Sheet 2 F/q; Z.

, z 4 R X ubumowc mm 0f 5 o 3% d M s .b w W z N .,..l| 1.. .m M z w m F f o WM V 1T. .m H

a w m fm@ .mouwwxmmvxmww Q KMNPSQ w .w W \\5 kwhtmt u x MM d M a 5 m 3 ,m a X. n a V Z d m o m\ z m mm m m ,z 3 m B Z.

gaand Group Jean Oum/'ef e Lavigne. Fou'h /'oup BY ATToRNEY.

Fell 4, 1941- J. L oUMlET ET L AvxGNE 2,230,253

SEPARATION OF LIQUIDS Filed Feb. 18, 1937 7 Sheets-Sheet 5 Conde/75er' and azenf Heat @cupe/afar Raw Paf/clem v Um/aPOr/zea kes/due Liga/'a7 a3: l Pump gr? f INVENTOR v Jean Oum/'ef e Lav/gne.

ATTORNEYS.

Feb- 4, 1941- J. I oUMlET ET I AvlGNE 2,230,253

SEPARATION 04F LIQUIDs Filed Feb. 18, 1937 '7 Sheets-Sheet 4 INVENTOR.

ATTORNEYS Jean aum/,er er Law/grua` Feb 4 1941 J. LouMlET ET LAvlGNE 2,230,253

SEPARATIONOF LIQUIDS Filed Feb. 18, 1957 7 Sheets-Sheet 5 Fig. 5.

INVENTQR. Jean Loum/e e Lav/gne.

ATTORNEYS.

Fell 4, 1941- J. LouMlET ET LAvlGNE 2,230,253

vSEPARATION OF LIQUIDS Filed Feb. 18, 1957 7 Sheets-Sheet 6 Hq, /3. ff ff i INVENTOR.

Jean Loc/mie# e Lav/gne.

BY www ATTORNEYS.

Fell 4, 1941- J. LouMlET ET L AvxGNE v 2,230,253

SEPARATION 0F LIQUIDs Filed Feb. 1S, 19:57 7 sheets-sheet" 'r Patented Feb. 21, 1941 UNITED STATES PATENT OFFICE Application February 18, 1937, Serial No. 126,401 In Cuba June 29, 1936 11 Claims.

This invention relates to the separation of liquids, especially to separation employing fractional distillation and fractional condensation by multiple eiIects, and more particularly to a novel process for accomplishing such separation, and it relates also to improved apparatus for carrying the process into effect.

An object of the invention is to accomplish the separation from a body of liquid comprising admixed uid constituents characterized by differences in volatility, of the several constituents, separating each according to its respective volatile characteristic.

A typical example of the useful application of the novel process herein disclosed is for the fractional distillation of petroleum, although this is only an illustrative use, as the process may be utilized in any eld for which it is adapted by the nature of my improvements.

Furthermore, the use of the novel process in conjunction with the process of centrifugal separation of vapor from entrained liquid forming the subject-matter of my co-pending application for United States Letters Patent, Serial No. 99,317,

filed September 3, 1936, presents notable advantages, which will be lexplained herein, but the utilization of the present invention is not dependent upon conjoint use with that process.

The novel process of the present invention, when viewed in its broad, or generic, aspect, provides for fractional vaporization of the mixture to be distilled by causing a stream thereof to ilow successively through a series of confined zones heated at temperatures increasing progressively from zone to zone, so that in each of the zones the more volatile constituents of the mixture flowing therethrough are evaporated. It is a primary object to provide for heating the increasing liquid in each zone, except one or more zones at the end of the series, by the transmission through such zone of the residual liquid from the hottest zones, which has not been vaporized, and the condensate from the higher temperature zone or zones, in addition to the vapor to be condensed from at least the immediately preceding zone.

The vapor returned to a zone from a zone of higher temperature for condensation transmits its heat of vaporization to the incoming liquid in the zone. In this way, the latent heat of vaporization is recovered. The condensation of the vapors, however, does not serve to recover the heat which has been put into the residual liquid (never vaporized) nor the heat contained in the 55 condensed fractions. The transmission of the residual liquid through all of the zones and the transmission of all the condensate from each zone through all of th-e lower temperature zones plays a very important part in the eiciency, economy and feasibility of the process. It makes 5 available for recovery in each zone the specific heat contained in all the liquid transmitted outward from the next hotter zone, in addition to the latent heat of vaporization contained in the vapors transmitted outward from the next hotter .10 zone. The fact that all of the heat, both latent and specific, is thus made available for recovery is of very great importance in enabling the fractionating to be carried out in a multiplicity of distinct steps. If thelatent heat alone were recovered, the heat required for raising the liquid fractions to their vaporizing temperatures would all be lost, and the number of fractional steps would be drastically limited as compared with the capability of the present process. 20

It is a further point that the recovery of the specific heat enables the successive zones or effects to be balanced against one another so as to maintain a substantially uniform temperature difference between the vapors undergoing con- 25 densation and the liquid undergoing Vaporization in each of the Zones, so that a suitably rapid rate of heat interchange can be maintained throughout. It is also an important point that the recovery 30 of specific heat can be so regulated as between the zones that the heat transmitted to the liquid in each zone may be properly proportioned to carry the thermal load of that zone in accordance Awith the characteristics of the liquid being 35 treated. One kind of petroleum for example, may be relatively rich in a givenfraction, and relatively poor in another, while in a second kind of petroleum this situation may be reversed. The provision of specic heat recuperators in the 40 several zones enables the extent of heat recuperation to be adjusted between the zones s0 that there will be relatively high recovery of heat in the zone in which a predominant fraction is vaporized and relatively low heat recovery in a zone in which a minor fraction is vaporized. The volatilization temperatures at equal pressures of the products of two successive zones will generally be too close to one another, when the fractional subdivision is very extended, to operate these adjacent zones under the same conditions of pressure, for the reason that there would be an insufficient drop in temperature as between the adjacent zones, to cause the interchange of heat between the vapors being condensed and the liquid being heated at a practically rapid rate.

It is accordingly another object of the present invention to provide for evaporation in the successive zones under pressures within the confined areas increasing step by step from one zone to the next. Provision for such increases in pressures may be desrably eiected by suitable increases in the gravity head of the liquid being distilled, as by mounting the zone containers in stages decreasing in height in the direction of input ow. Alternatively the circulating mixture may be pumped from one zone container to an'-V other.

paratus, and also because it requires the least pumping effort. The disposition ofthe zone containers at heights which are successively greater from the last to the rst in the systenr,l requires that the entire body of liquid to be heated and vaporized must be pumped tothe level necessary to provide an adequate gravity head and consequent pressure in the system.

In thisI connection it should be noted that the diierence `in temperature between the condensation of the heating vapor and that ofthe liquid which isv evaporated in agiven zone by the heat (derived from such condensation) Varises from two causes: on the one hand, the greater volatility of the bodies which are evaporatedas compared with those which are being condensed: and onthe other hand the diiference of pressure,V for the regulation of which provision is made as already indicated briei'l-y'and which will be described more at length hereinafter.

In pursuance of the invention, -another object is to provide an improved apparatus by which to carry into effect the novel process whose objects and features have been summarized-brieily in the foregoing paragraphs.

Other objects and features will appear ast-he description of the particular physical embodiment selected to illustrate the invention progresses.

In the accompanying drawings, like characters 'of reference havev been applied tocorresponding parts throughout the several viewsI which make up the drawings, in which:

Fig. 1 is a schematic view in front elevation of part of an apparatus for the fractionall centri'fugal distillation of petroleum adapted to carry the invention into eifect, and in the construction of which the present invention has been embodied;

Fig.2 is a View similar to Fig. 1, and illustrates a continuation of the distilling apparatus of Fig. 1, from left to right;

Fig. 3 illustrates similarly a continuation of the distilling apparatus of Fig. 2, from left to right; y

Fig. 4 similarly illustrates a terminal portion of the apparatus of the preceding figures, being in continuation of Fig. 3 from left to right;

Fig. 5 is a view in horizontal sectional detail taken on the line 5 5 of Fig. 1, the arrows at the end ofthe line indicating the direction in which the view is taken;

Fig. 6 is a similar horizontal sectional detail on the line 6-6 of Fig. 1;

Fig. 7 is a horizontal sectional detail on the line 1-1 of Fig. l;

Fig. 8 is a horizontal sectional detail on the line a-a of Fig. 1;

Fig. 9 is a fragmentary detail view in plan of the heater R shown in Fig. 1, taken separately;

This second, or dynamic, mode of prof cedure is regarded as more advantageous, both because it facilitates the installation ofthe ap- Fig. 10 is a similar detail view in plan of the heater R3 shown in Fig. 2, taken separately;

Fig. 11 is a detail view on an enlarged scale of a typical cross-section of the helical tube component shown in Fig. l5, and this figure shows also a diagram of forces;

Fig. 12 is a fragmentary detail view in vertical longitudinal section of a portion of the helical tube structure shown at the lower partvof Fig. 15, with part of a liquid-collectingtube connected thereto; l vFig. 13 is a schematic View illustrating in ilowsheet form a series of air traps, with their associated ducts;

Fig. `14- is a detail View in vertical section, on an enlarged scale, of an air-trap of the type shown-'in Fig. 13;

` Fig. 1'5A is a fragmentary detail View in vertical-section, somewhat schematic in character, ofua modified form of helical distillationl tube and associatedextraction or collcting tube for the liquid prod-uct; v

Fig.V 16 shows a modified-system. f

In a now-preferred embodiment of the invention selected forilllstration and description; and referring first more particularlyto the-struc# ture shown in Figs. l to. 4, inclusive, an? apparatus is there illustrated intended for the fractional distillation ofpetroleuni by multiple'eiects; and in whichl provision is shown'for dividing the vapori-zation and condensation, each intdfolir frac-` tional steps, although it is to be understood that where desired a division into si-Xgeigl'itl o'i"n1ore fractional steps may be eiec/ted,v or; on thelcontrary, the'divis'ion can b"e reduced tor two or three operations.

Where; the distillation irivlves Operations' to vfect separation of its various constituents;- but the cost of installationis greater. t

In the apparatus vnow under'des'cription, the heating,4 vaporization and condensation are carried out' in a ser-ies of zones coniifnedwithin contain'ers', the reference characters Tf, T2, T3, T4 and 'IE5 designating generally the containers and the zones respectively conned thereby. Before describing their structural details, the iiw of mixture vnirougn the-system wilt seldescribed with suflicient detail to permit av ready understanding of the novel process.

The raw petroleum enters the System through a suitable duct A4 (see-Fig. 3), and; after" being heated in a-heatrR, this liquidspply stream enters the heaterT at its lower part where indicated by the arrow point from' which a lead line runs to the reference character Il tf1-tg. 3, it being understoOd that the illustration this respect, as in general,` is of a schematic character whenever the operation can be sti-indicated the rising-*liquid to travel in a helical path. The' liquid is heated as it traverses this path in contact with the exterior of the coil S4. The coil S4is almost hot enough to cause vaporization ofthe rising liquid to occur.

'Ihe rising liquid leaves the cOntainer T4 at the vent I4 and passes through duct A3 to the pump or impeller B3 by which it is vimpelled through continuations of the duct A3 and through heater R4 (see Fig. 2), to a point I4 where it is injected into the lower end of zone container T3. Therein it rises through a helical path Z3, defined, as in T4, initially by helical extraction coils I5, and then through a continuation of said path defined by the convolutions of a heating coil S3.

Vaporization is initiated continuously at the lower end of path Z3 and proceeds during the upward ow through that path and the continuation thereof along coil S3, the more volatile hydrocarbons being evaporated en route and then after their accumulation in the space T3, they pass out through duct X4 to heater T4 (see Fig. 3), entering the heating coil S4 therein to act in heating the original raw fluid supply as it iiows up the spiral path dened by the convolutions of coil S4 in the manner already described.

After running through container Zone T3 the vpetroleum goes out at I3 through duct a2 to defined by collection coils designated generally I1,

and around the convolutions of heating coil S2, being deprived in said path, and in the space T2, of the more volatile hydrocarbon constituents which it may still contain. These pass through duct X3 into the heating coil S3 of zone container T3, in order to heat the mixture rising in the helical path defined by convolutions of coil S3.

At the upper part of container zone T2, the residual petroleum comes out through I2 into a duct a' and its ow may be traced thereby through pump B' and heater R2 (see Fig. 1) into the lower part of zone container T' atpoint I8. Therein it rises, as in the preceding container zones, along the convolutions of the collecting coils I9 through the helical path Z' to the continuation thereof formed by the convolutions of heating coil S', evaporating, inthe course of its travel, and in the space T', the hydrocarbons of vgreater volatility remaining in it, which vaporous product comes out through the space T' into the duct X2 and through it into the heating coil S2 of container zone T2.

Finally, the petroleum issues from container T' through opening I' Ito duct a and passes therethrough and through pump B and heater R into the tubes of a boiler H where the least volatile vapor fraction desired is driven off, this boiler constituting the last zone and the only zone which is heated directly. The vapors produced in the boiler are condensed in the coil S of the penultimate container T', causing therein the evaporation of less dense products, which, in turn, upon their condensation in the coil S2 of the container T2, evaporate the less dense products in it, and thus, in succession, on to the first container zone of the system, in this instance T5.

Further features of novelty in operation of my improved process of Adistillation will appear in connection with the following description of the apparatus as illustrated in the drawings.

The boiler H comprises upright tubes`20 disposed in vertical coils which stand one behind another when viewed as in Fig. 1, and the arrangement of which is shown clearly in the sectional views 5 to 7 inclusive.

The horizontal tubular components 2l of the coils, which connect the upper ends of the tubes 20, ar-e situated in the plane of Fig. 6, and each tube 20 has an extension 24 above the plane of the cross-connections 2| to the plane of Fig. 5, in which latter plane are disposed manifolds 22, to receive the vaporous output of the tubes 20, 24, delivering it through a common cross tube 23 to the duct X which delivers it to be condensed in, and to heat the coil S' of Zone container T in the manner already indicated.

It may be assumed that the petroleum does not become completely evaporated in the 'course of the distillation, and that approximately a fourth part is available in the form of a hot liquid which can be and preferably is, used to heat the heaters R', R2, R3, R4 and R5, in the order named, its course being traced from the point 29 at the bottom of boiler tubes 20 in Fig. l, through duct 30, and duct 3| in heater R', etc., through ducts 33, 34, 35, 36, 31, 38, 39, 4U, 4I and 42, to the refrigerator element R6, where it is cooled, if its viscosity will allow such cooling.

The vapors produced in boiler H ow through duct X' into the coil S and their condensation in that coil is effected at a temperature higher than the temperature of evaporation of petroleum circulating in T', not only because the petroleum gives oi in that zone more volatile hydrocarbons, but because the pressure within the coil S' is greater than that within the zone T. Such conditions favor the transmission of heat between the vapor circulating in the coil and the liquid which surrounds it; and by virtue of such efficient transmission the condensation in the lrst and the evaporation in the second are promoted.

Moreover, some slight part of only relatively volatile hydrocarbons might possibly resist evaporation in zone T', and consequently might be found in the vapors produced in H which go through S'. Those hydrocarbons ldo not condense in S', or do so with diii'iculty, and in order to provide for such a contingency, the ylower terminal Sm of coil S' is connected, as by a duct b with the duct X2 which carries to coil S2 the vapors produced in zone container T'.

As already mentioned, a lower pressure prevails in the coil S2 and by means of such a pressure differential, which may be regulated by a cock UI in duct b, and `by a cock V' in the duct X2, the velocity head of the vapor as it passes through coil S' may be regulated. In turn, the pressure in the zone container T' is controlled b-y regulation of the impeller operations (B, B' etc.), and by the cock V', and in the same Way the various pressures which it may be desirable to maintain in the zones T2 and T3, and in the boiler H, may be controlled and regulated.

The condensation within` coil Si' is eiected progressively from top to bottom, beginning with the less volatile hydrocarbons, because the cooling becomes established progressively. Owing to the flow upwardly of the petroleum which cools the coil, the temperature of that petroleum is higher in proportion to its level, and consequently the uid being condensed is subjected progressively to a cooling fluid of ever diminishing warmth.

At the same time, also, the pressure in the coil keeps diminishing slightly, and both of these conditions favor the progress of the condensing operations .all along the coil; Such progressive con-l densation lquenes: continuouslyV and; successively,

in the vo rclerof their progressivelyv lesser volatili,-Y

ty, the hydrocarbons containeddn' then; vapors: whichmravel inthe coil.l As they'become liqueed,.the `centrifugal. force to which they, are sub--V jected; by their tortuouspro'gress.- at high speed througlfrthel helical coil keeps driving thennto- Wardl the exterior Wall of the small gathering channel'formedfby., the outeri inferior. endof the coil section,l.where.they are collectedat intervals, The cross-sectional areaof the bore of the coil is decreased. gradually,`or by steps, in order to compensate .for the. decrease involume of fluid as the result of condensation. Asuitable structure for this purpose is illustratedin Figs.. 11, 12 andfl5Y of the drawingsv in. which the. tubular elementf-isidesignated generally S. In the'diagram of forces inFig. 11, the arrow'indicates the resultant oi centrifugalland gravitational for-ces, the horizontal component C representing the moment of centrifugal force while the VerticalV component. G'represents the gravitational moment.

Itmay be noted that while onlyilvecollections of extractionsfor each coilfhave been shown in the present instance, the greater the number of such extractions the more fractional will be the petroleum output.

The collecting pipesV-Z--ZX respectively start tangentiallyy tothe convolution from which each springs, as shown at OZv inFigs. 12and15, but, as indicated clearly in the last-named-gure, at A0, theyy keep curving and` changing their direction until they become vertical, bengdisposed in contactwith ythe inner surface of the exterior Wall of the container at the regionof such curvature (see ZZ, Fig. i', etc.).\ They departl from the straight.. reaches,y as. .ZZ,v When theyV reach: the bottoni oi' the coil,- as at the plane of the section line S-f, (see l1) and at this region they are assembledv inrnultplc transversely of they annular space, as Z', in which they follow a. helical path downward.; the lower terminals of these.heli cal collection tubesbeingeled out through suitable openings inthe bottom of the container, as at a to e5 inclusive.

This assembly of collectingl tubes occupy substantially the. entire annular. space Z', andtheir disposition and. surface Acharacteristics conform to then/ecessity of .transinittingthe entire availahleheat7 within .practical limits,A frein-the .liquids flowing inthe collection tubes. to the circumjacent helical stream ofpetroleurntobe distilled, frornthe moment of. its entrance .to the rstcontainer Zone, as at l8- iniFig. l.

After. issuing from the zone container Tiand after. previous separation of. thefvaporsr which may be entrained by the* liquids. circulated 50 through the vapors,-.the collecting.pipesY z-e in elusive contribute successively-.to the heating of` petroleumin-thefreheatersdR3, Rland R5, and are afterward cooled, as by water, in R5 before barreling or storing the products which they carry.

The present process of fractional vaporization and condensation with multiple effects does not require for its application that precisely the same quantity of heat he applied in each one of the successive fractionatings.

If; for example, it is desired to reduce the distillation operation performed in a zone because thev petroleum treated containsY a smaller quantty of hydrocarbons corresponding to the group which it is desired to evaporate. in that zone, Vit

willA be l sucent. to reduce. the-V heating surfaceof-the .heat recuperators:otthatzonaI and thereby reduce the recovery of vheat `in\ the` zone. Asa compensation, however, that heat .not recovered in the zone referred to is. additionally available for therecovery. inthe next colderv zone, or in any of the colder zones as desired.

In order to effect the separation of the vapors entrained with. each of the extracted liquids, provisionjis. made in each of the extraction lines a--25, etc., ,of an trap similar tojthat shown atv AT. in.Figs. 13 and l4roflthe drawings,

The outlet'. forf vapor from the first trapjis shown at f in Fig. 14, and is connected by the duct f leadingto the coil S2-of the next follow-1 ing container, in which a lower pressureprevails. The vapor is `thus inspired.` into. the system, free frominspiration. of liquid, which collects. in the spaceSP of the trap, andnmay bewithdrawn from the. trap, asat y. in Fig. 14.. ,I f liquid rises in the trap to an undesired height, the vioat FY rises thereonand. shuts off the duct f automatically;

Fig. 13 illustrates in HOW-form an assembly of traps, like AT, associatedWith a systemof ducts in which the reference. characters z-eA .designate the dischargepipes, While the vapor outlet-duct f has branches ff, f2', f3, f4 and fE-leading each to. the air outlet` of one of the traps. The traps derive. the collected fluid from the ducts leading respectively from the bank ofhelical coils Z".

In the same. way thatthe vapors produced in the boiler. Hfeedthe` coil Sl andv induce the evaporation of the more rvolatile productsofthe petroleum-.Which runsthrough tank Tf, those products of`tank..T, Whenievaporated, feed the coilv S2 and induce. the evaporation of the more volatile products i of' the petroleum running through tank T2. The endI ofthat coil S2 remains connectedlwith coilSS which is at a lower pressure andf in consequence inspires the vapors from S2', inducing. inthe coil the speed of those vapors which is regulated by. the cock U2.` The vapors not'. condense'd'in S2A are thus condensed in coil S3`atl lower pressure and temperature.

The. operations in container zone T2' arecar-v ried out in thesame Way as described for container zone T'. After issuing'f'rom the container zone T2, the. collectingV pipes for the' condensed liquids, once deprived of` the vapors entrained -by those liquids, heat the re-heaters R4 and R5 andare afterwards cooled' in Rwith coldwater, before theproducts Which they carry are bar# relled.

The vapors produced in T2"a`re carriedin turn to coil' S3`Which heats taiilr'la and induce the evaporation rof the more volatile'productswhich run Vthrough that tank,.namely the raw'petroleum.. y Iii th'atltank. T3'the naphtha is evaporated..r The end-of S3 is Vconnected with the coil Sdvvl'iichY heats the petroleum'which circulates in the heaterLC which is at' a lowerpres'sure', the speed'otheivapo'r in coil'SSfinduced by that difference of I pressurebeing ,regulated by the stopcockU3`. The vapors not" condensed in S3 are. thuscarriedto coil Sd which; operates at alovver: pressure. i

The. :operat'ins in tank"` T3`are. eiectedin the same'way.. as .in .T Y'fadiTl The .collection pipes of the liquids condensedlinithatltanlgwhenfissuing.5 from.. the. sameand thedfagged' vapors havingfbeenlseparated; .heat the. heater: RBT. and are ait'enwarda cooledwitl-i` coldlqwater: in the cooler Rlbeforerliarrelingythe productswhich 1 Iso fili

iinitesimal entrained drops. aration'practically no bodies of less Volatility are .condensable gases that might exist, that passage Abeing regulated by the cock V4.

The passage of the vapors through all the successive coils is effected owing to the difference -of pressure between the boiler and the atmos phere, and regulating the successive increases of the pressures in the various tanks by means .of the cocks V, V', V2, V3, V4, U', U2, U3 and U4.

The coils and the I'pressures are determined so that with the difference of temperatures v'existing between the heating vapor and the heated fluid, the transmission of heat through one coil shall correspond to the amount of evaporation required to maintain the velocities of the vapors in the coils suiiiciently high to correspond with 'the necessities of the separation, and' so that the loss of pressure by the passage of the Vapor at that velocity in e'ach coil shall represent the dif- .ference of pressure existing between two "successiv'el'y connected container zones.

The collection pipes of liquids condensed in the coil of the heater T4 are arranged similarly to those of the collecting pipes in the tanks T', T2 and T3, and in the lower part of that heater they heat the petroleum to be distilled. When issuing from that heater and after previous separation of the vapors entrained by them, they proceed to the cold water cooler R6, and afterwards tothe barreling stage.

The collection pipes of the liquids condensed in coill S4 are directly conveyed to the cold water cooler R5 so that these liquids become cooled before being barrelled.

The mechanical separation, which is effected by means of centrifugal force, in the various coils of that apparatus, 0f the liquid which keeps condensing in them, and in the measure that that condensation is effected, constitutes the novel method of distillation disclosed and' claimed in my co-pending application, Serial No. 99,317.

In principle, we must admit that the aforesaid mode of operation is not perfect, and that the progressive condensation of a mixture does not, in a strictly absolute manner, liquefy its components according to their volatilities; because before one hydrocarbon has .been exhausted in the vapor mixture, the condensation of another more volatile hydrocarbon has been initiated.

That obstacle to the attainment of a perfect analysis is reduced in centrifugal condensation, because the'latter does not encounter the fact characteristic of every other method of distillationv that a less volatile body will exist united with more volatile vapors, as much in the vapor state as in the liquid state, in the state of in- In centrifugal sepentrained in the liquid state by less volatile vapors, because the whole of the liquid is separated Vby centrifugal force.

The analysis of the products is improved in centrifugal separation by employing a feature of the process of my Vinvention as disclosed in rmy co-pending application Serial No. `116,333,

filed Decemberl'?, 1936. Said feature consists Ain subjecting the liquid to the heating action of friction developed in a thin andpreferably rugose channel for the yliquid separated within the channel of a coil having approximately the typical cross-section illustrated in Fig. 11 of the presentv application. Such rugosity is indicated at Sr in Figs. 11 and 12. The friction there produced by the flowing vapo-r is thus increased, consequently inducing a rise of temperature which heats the separated liquid and evaporates its more volatile components, driving them back toward the interior of the coil. As that friction is due to work performed by the circulating vapor, consequently the performance of that work is accompanied by an equivalent decrease in the heatenergy which the Vapor possesses. Such decrease of heat-energy is accompanied by a condensation which is caused by the cold produced in the interior of the uid, and which, in its liquefying effect, must select the less volatile hydrocarbons more efficiently than the exterior cold which is transmitted by contact; since the latter affects directly only the layers which circulate along the walls.

I have found that by means of the friction induced in the small channel for the collection of the liquids separated in the coil, two rectifying effects are obtained in that coil. First a rectification of the circulating vapor, by the condensation of its less Volatile elements. Second, a rectication of the separated liquid, by the evaporav 'tion of'its more volatile elements. The application of that invention can, therefore, be advantageously effected in conjunction with the new novel process herein disclosed.

'I'he 'foregoing description is intended to disclose a particular application of the process; but, of course, many details are susceptible of modification.

I ,wish particularly, to point out the possibility of dividing the distillation container zones into two series; the container zones of one series alternating with those of another in such a'way that if the containers are numbered inthe order in which the mixture to be distilled runs through them, the even numbered containers belong to one series and the odd numbered containers belong to another series.

So, also the boiler which ends the distillation of the petroleum may be divided into two boilers or tanks, one heated by the gases from an oven and the other, at a lower temperature, by water vapor at high pressure; and the multiple effects areestablished only between one of the boilers and the containers of the same series.

For instance, if the installation comprises 8 tanks and two boilers, one of them heated by vapor, the boiler heated by a furnace and tanks 8, 6, 4 and 2 will constitute a group of quintuple effects, and the second boiler, heated with vapor will constitute in conjunction with containers 1, 5, 3 and l, another group of quintuple effects, independent of the rst; and it is contemplated that the temperatures of the successive tanks from 8` to I shall decrease with suitable and continuous regularity.

This system is illustrated in Fig. 16. The petroleum enters through tube 5l) and by means of the pumps 5I it travels successively through the unitsor zones 52 to 58 inclusive and through the two primary heaters 60 and 6I, one of which BI being heated by a furnace and the other 60 being heated by steam.

Each unit 52 to 59 inclusive is the same in 'construction and operation as the units T shown in (Figs. 1, 2 and 3. The vapors generated in the heating ,zone ..60 ,passby .tube;63 into the unit 4or zone l.58,.supplyingzheat Y.to the liquid therein :for vaporization, theentering vapors' being subjected to fractional condensation. The vapors .generated in unit 58 passYby-its-tube 63 to zone56. It

will .now be understoodthat the vapors-generated -I .have described what I believe tobe the.best l embodiments of my invention. I' do not however, to b e 4vconfined to the embodiments SlOfwn, buter/hat I desileto cover by; Letters Patentis set; forth in the appended claims.

I claim:

1. Thamethod of .distillation .which comprises providing a single primary heating zone, ,transmittlng the liquid tobe distilled towardthe primary heating .zone for progressive heating and vaporzation through `a successionof zones maintained at successively higher pressures and Ytemperatures, including the ,passing of the unvaporized residue of .eachzone Von to thenext hotter zone, andfinally to the` primary heating zone, re turning the vaporized .product of each zone to the neXt colder zone for condensation therein, passing the vapor to be condensed-in each instancethrough the zone in which it\is;to be condensed in the opposite direction to the flow of liquid through such zone, while maintainingrthe outgoing vapor and vtheincoming liquid separate but in'intimate heat exchanging relation, and

passing the outgoing unvaporized `residue from the primary heating zone and the condensateY from each zone into heat exchanging relation lwith the incoming unvaporized liquid as theunltioned-in -a desired relation appropriate tov-the heating and vaporization A.to benperforrned in the .respective zones, ythe pressureincrease from zone 'to zonebeing sufcientin each instanceto bring Aabout asharp difference of temperature between the vapor-fraction.evaporated in `a-zone of higher ,temperature and pressure, and the liquid'to be` evaporated in the zone of next lower temperature `YAand pressure, whereby the rapid and economical transferenceiof heatfromsuch vapor to such liquidiiseiected 52;-71'he process ,of fractional distillation by lmultiple, effects, as claimed in claim 1 in which laltent heat of vaporization is .appliedtothe riuid stream in one or morelzonesby a `counter viowy therethroughof vaporous products, Vin coni-lnement to atoltuouspathwithin the zone or, zones,

.whereinthe vaporous products .are subjected to separating actiombyithe resultant 0f centrifugal forcefandegravity.

,3. The process of fractional distillation byv multiple effects as claimed in claim 1, in which latentheat4 of ,vaporization isapplied'to the 'fluid Stream in oneorimore zones by a counter flow therethrough of vaporous products travelling at high ,velocity in con-iinement to a tortuous pathv of gradually decreasing capacity within each zone, wherein these vaporous products arel subjected to separating action.byfthe resultant of ycentrifugal forceand gravity, whereby condensationof the vaporous constituents of said counter-,owing v ai pors supervenesin proportion inverselytozthe relative volatility of the several constituents, andas those condensed liquids come into being theylare projected against the walls ofY the. conningstructureilbyrthe centrifugal -force, andare collected and extracted for further disposition.

' l4.@The process of fractional distillation @by multiple effects vasvclairned in claim v1, in-vvhich latentl heat of vvaporization is` applied to the 'fluid streamin oneor Amorezonesloyaal counter-How therethrough of vaporous products travelling atv high velocity, sin confinement tofa `tortu'ous path of gradually decreasing capacityfwithinreach zone, Vwherein vthese-vaporous productsare subjectednto separating actioniby the `resultant of centrifugal force and gravity, `whereby Ycondensation Aof the vaporous constituents ofsaid counter-flowing-.va-

pors supervenes in proportion inversely tov the, relativevolatility of the several constituentsand as y those condensed liquids comezinto-being theyare projected against the walls of. the` confining structure by the centrifugal force, and are` collected and extractedfor further disposition, andfwherein the uncondensed vapors-,are transmittedI to the next colder zone for further condensation.

:5. :The process of fractional distillation by vmultiple effects as .claimed in claim` 1, r`in which latent heat of vaporizationgisapplied to theffluid stream in one or `more zonesrb'y-a counter flow therethrough of vaporous products, `in confinef Amentv to atortuous path withinA the zone or zones,

.wherein theyfarelsubjected to ,separating actionlbythe resultant of centrifugal-force'andfgravity, and wherein the separated, condensed'liqud is caused to=travel invcontact with a rugose 'surface -for promoting rectification.

l6. A process of fractional separation of petroleum involving Vfractional vaporization and fractional condensation, in which the petroleum- Fto be vaporized is caused to travel progressively through successivezones whereithe-several frac- 65 tional vaporizations take place in ascending temperature and pressa-reorder, and all the products of the distillation including the vapors produced' tok Vin each fractional vaporization, `the condensate f of those vap'ors,vand the final residuevliquid are 60 e caused to run in a contraryor inverted direction and order through the colder fractional vaporization Azones where they -are utilized as heating iiuids to'heat the petroleum'to'bevaporized and the pressureincrea'se :from Vzone to zonebeing sumucient in -each instance to bring about a sharp dif- Yresidue and condensate'liquids issuingvffrom the zone of next higher temperature and the latent heat of vaporization contained in the vapor which issues from the zo-ne of next higher temperature are delivered (excepting the outside losses by cooling caused by the surrounding air), the whole of the heat provided in the zone of highest temperature being transmitted to the second zone and constituting the only means for vaporization of the 1iquid in the second zone; and the whole of the heat contained in the residue and condensate liquids and in the vapors issuing from each zone constituting the only means for vaporization of the liquid in the zone of next lower temperature and being totally transmitted to such zone of lower temperature, (excepting the outside v losses), there being thus maintained through its successive re-employment in the several fractionatings a uniform quantity of available heat for each one of those operations, (excepting outside losses) whereby the thermal equilibrium of the operations in the several zones is attained; the liquid being heated as it passes through the several zones toward the zone of highest temperature being subjected first to heating by the residue and condensation liquids and then by the vapors from the next hotter zone; the total quantity of heat put in the liquid in the several zones being allocated or apportioned by regulating the heat exchanging capacity between the liquid being heated, on the one hand, and the residue and condensation liquids on the other.

7. The fractional distillation process consisting in the establishment of a primary zone heated l by outside means and a series of secondary zones 35A 'of progressively lower pressures starting from the primary zone, and said zones being successively travelled by the operated liquid from the last y one down to the primary one; in which course the liquid is heated and vaporized by the calefac- 40 tion brought on to each-zone by the vapors distilled in the anterior zones, by the residue which runs through all those zones in counter-current to the operated liquid and by the condensations produced in each zone which also run at counter- 45 current to the operated liquid in each one of the zones posterior to that in which they were produced; to which effect the operated liquid is maintained in all those zones successively o-r simultaneously in heat exchanging relation but out of 50 contact with the said heating fluids and the motion of the operated liquid from one zone to the following one is elTected by pumping to secure a regulated increase of pressure from zone to zone and thereby to secure an ecient difference of 55 temperature in each instance between the liquid to be evaporated and the vapor which heats such liquid.

8. The process of fractional distillation consisting in providing a plurality of primary heat- 6o ing zones heated by outside means, and for each one of those primary zones a series of secondary zones with an equal number of zones in each series; in causing the operated liquid to run through that succession of zones so as to interpose between the connections between two successive secondary zones corresponding t0 one primary heating zone, one secondary zone of each one of the other series; in which course the operated liquid is raised in temperature and evaporated by the heat which it receives in each zone from the vapors produced in the anterior zones of the same series those vapors ilowing exclusively through the zones of their own series in inverse direction to that of the operated liquid and becoming condensed in the same; also by the heat which the opera-ted liquid receives from the residue which runs through the successive zones at counter-current becoming gradually cooled in the same; and by the heat which said operated liquid receives from the condensations of the vapors that are condensed in the secondary zones and run at counter-current through the zones posterior to the zone in which they were condensed; and in each secondary zone the transmission of the heat between the vapor which is condensed and the liquid which is vaporized is effected by maintaining both fluids in heat exchange relation through a metallic wall, and the transmission of heat from the residue and from the condensations to the operated liquid which is heated is also effected in a similar way.

9. A process as described in claim 8 characterized by the fact that the successive zones traversed by the liquid are at pressures higher by steps, the pressure increasing in the direction of the motion of the liquid; those pressures being established by the pumping of the liquid from one zone to the following one.

10. The combination of the process described in claim 7 with the fractional condensation and separation process. which consists in causing the vapors undergoing condensation in each zone to travel at great velocity in a helicoidal path of progressively diminishing cross-sectional area to separate the condensate from the vapors, and in withdrawing the condensate from the vapors at intervals along such path.

11. The process as described in claim 8 characterized by the fact that the successive zones traversed by the liquid are at pressures higher by steps, the pressure increasing in the direction of the motion of the liquid, those pressures being established by the pumping of the liquid from one zone to the following one, and further characterized by the inclusion of the fractional condensation and separation process which consists in causing the vapors undergoing condensation in each zone to travel at great velocity in a helicoidal path of progressively diminishing cross-sectional area to separate the condensate fro-m the vapors, and in withdrawing the condensate from the vapors at intervals along such path.

JEAN LOUMIET Er LAVIGNE. 

